CN109742377B - Method for surface modification of high-nickel ternary positive electrode material - Google Patents
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention provides a surface modification method of a high-nickel ternary cathode material, which is characterized in that the high-nickel ternary cathode material is placed in a plasma generator, carbon dioxide gas is used as an arc striking gas, the surface of the ternary cathode material is treated in the atmosphere of the carbon dioxide plasma, and a lithium carbonate layer and a carbon coating layer can be built on the surface of the ternary cathode material in situ, so that the direct contact between an active substance and electrolyte can be effectively isolated, the electronic conductivity of a surface interface of the ternary cathode material is enhanced, the chemical stability of the ternary cathode material exposed in humid air for a long time can be greatly improved, and the structural stability and the post-processing property of the ternary cathode material are improved. The ternary cathode material surface treated by the method is rough (tree root-shaped), and the processing performance, the cycle stability, the capacity retention rate and the rate capability of the ternary cathode material are obviously improved. The surface treatment method has the characteristics of simple process, simple and convenient operation, rapidness, high efficiency, low cost and remarkable economic benefit.
Description
Technical Field
The invention relates to a surface modification method of a high-nickel ternary cathode material, belonging to the technical field of lithium ion battery cathode materials.
Background
Lithium ion batteries have been widely used in portable electronic devices, household appliances, and power tools. However, the application in the field of electric vehicles has not achieved such achievement, mainly because the high cost of the lithium ion battery increases the cost of the electric vehicle, and the specific energy density does not meet the use requirements of users, which limits the development of the electric vehicle. Currently, the cost and energy density of lithium ion batteries are largely dependent on the performance of the positive electrode material, which is the heaviest and most expensive component. The high-nickel ternary cathode material has the advantages of high mass specific capacity, low price and the like, and is considered to be the cathode material of the next-generation lithium ion battery and has received wide attention. However, the high-nickel positive electrode material is very sensitive to water in the air, and is very easy to react with moisture in the air to generate lithium hydroxide on the surface, so that the surface of the material is deteriorated, and a plurality of problems of difficult preparation of subsequent positive electrode slurry, poor positive electrode capacity attenuation, poor cycle stability and the like are caused. Therefore, the high-nickel anode material without surface treatment has more strict requirements on storage conditions and later processing environment, so that the storage cost of the material is increased, and the subsequent processing difficulty of the material is also increased. In order to solve the above problems, researchers often modify and decorate the surface of the high-nickel ternary cathode material by using an inert oxide coating method, so as to improve the structural stability and the cycling stability.
Chinese patent CN106207128A discloses a Zr (OH)4The preparation method of the nickel-cobalt-aluminum-coated ternary cathode material comprises the following steps of: (1) preparing an alcoholic solution of a soluble zirconium alkoxide; (2) preparing an alcohol-water solution, and slowly dripping the alcohol-water solution into the solution prepared in the step (1); (3) ultrasonic treatment, washing, suction filtration and drying to obtain amorphous Zr (OH)4Powder; (4) mixing ternary material with Zr (OH)4The powder is mixed by ball milling to obtain Zr (OH)4And coating the modified ternary cathode material.
Chinese patent CN103178258A discloses a preparation method of an alumina-coated modified nickel-cobalt-manganese ternary positive electrode material, which comprises the following steps: (1) preparing a precursor: preparing a mixed solution of water-soluble metal nickel salt, cobalt salt and manganese salt, dripping the mixed solution into a reaction container together with a precipitator and a morphology control agent, controlling the pH value and the reaction temperature of the system, and filtering, washing and vacuum drying the mixture after reaction to obtain a precursor; (2) preparing an alumina-coated precursor: dispersing the precursor, water-soluble aluminum salt and dispersant in deionized water, heating while stirring until the dispersant is hydrolyzed, and filtering to obtain Al (OH)3The coated precursor is placed in a sintering furnace to be roasted to obtain Al2O3A coated precursor powder; (3) mixing Al2O3And uniformly mixing the coated precursor powder with lithium salt powder, and calcining at high temperature to obtain the aluminum oxide coated modified nickel-cobalt-manganese ternary cathode material with a layered crystal structure.
As mentioned above, the surface coating modification method for the high nickel cathode material mainly includes solid phase coating sintering and liquid phase coating sintering. The coating layer obtained by the solid-phase coating sintering method has poor uniformity, the bonding force between the coating layer and the matrix is weak, and the coating layer is cracked due to anisotropic volume expansion of the anode material in the circulation process, so that the material is continuously deteriorated, and the circulation performance of the material is influenced. Most of liquid phase methods adopt water as a solvent, however, water reacts with the high-nickel ternary cathode material to cause lithium loss, and finally, the capacity of the material is reduced. Aiming at the problems of poor coating uniformity of a solid phase surface, capacity loss caused by liquid phase coating and the like, the invention provides a plasma surface modification treatment method, wherein a lithium carbonate and a carbon coating layer are constructed in situ on the surface of a high-nickel ternary cathode material in a gas-solid reaction mode, so that direct contact between an active substance and an electrolyte can be effectively isolated, the electronic conductivity of a surface interface of the high-nickel ternary cathode material is enhanced, the chemical stability after the high-nickel ternary cathode material is exposed in humid air for a long time can be greatly improved, and the structural stability and the post-processing property of the high-nickel ternary cathode material are improved. Compared with the traditional coating method, the method has the advantages of simplicity, convenience, rapidness, high efficiency, low cost and the like.
Disclosure of Invention
The invention provides a method for modifying the surface of a high-nickel ternary cathode material to overcome the defects in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for modifying the surface of a high-nickel ternary cathode material comprises the following steps:
s1, paving the high-nickel ternary positive electrode material in a container, putting the container into a plasma generator cavity, starting a vacuum pump, and vacuumizing the plasma generator cavity;
s2, introducing dry arc striking gas into the cavity, maintaining the air pressure of the cavity at 500-700 Pa for 20-60S, and then extracting the arc striking gas to maintain the vacuum degree of the cavity at 40-50 Pa;
and S3, starting the plasma generator, adjusting the power, and reacting for 0.5-120 minutes to obtain the surface modified high-nickel ternary cathode material.
Preferably, the chemical formula of the high-nickel ternary cathode material in step S1 is LiNi(1-x-y)CoxMyO2Wherein x + y is less than or equal to 0.7, and M is Mn or Al.
Preferably, the chemical formula of the high-nickel ternary cathode material is LiNi0.9Co0.05Mn0.05O2、LiNi0.8Co0.1Mn0.1O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.85Co0.1Al0.05O2Or LiNi0.5Co0.2Mn0.3O2。
Preferably, the arc striking gas is carbon dioxide.
Preferably, the tiling thickness of the high-nickel ternary cathode material in the step S1 is 0.3mm to 10 mm.
Preferably, the power of the plasma generator in the step S3 is 5-2000W.
The application also provides a lithium ion battery, and the positive electrode material of the lithium ion battery is the surface-modified high-nickel ternary positive electrode material prepared by the method.
The invention has the beneficial effects that:
a layer of lithium carbonate and carbon composite coating layer can be constructed on the surface of the high-nickel ternary positive electrode material by adopting plasma surface treatment, and the lithium carbonate is an electrochemical inert substance, so that the high-nickel ternary positive electrode material can be isolated from water vapor in the air, and the lithium hydroxide generated by the reaction of the lithium carbonate and the water vapor is prevented from damaging the surface interface structure of the lithium hydroxide, thereby improving the processability of the lithium hydroxide in the subsequent electrode plate production process; meanwhile, the small amount of carbon in the coating layer can improve the surface interface electronic conductivity of the high-nickel ternary cathode material, and is beneficial to improving the cycle and rate performance of the battery; the method has the advantages of simple process, convenient treatment, rapidness, high efficiency and remarkable economic benefit.
Drawings
Fig. 1 is an SEM image of the modified ternary cathode material obtained in example 1;
FIG. 2 is an XRD spectrum of the modified ternary cathode material obtained in example 1;
FIG. 3 is a graph of the first three charge and discharge curves at a current density of 20mA/g for the battery prepared in example 1;
fig. 4 is a charge and discharge cycle curve of the battery prepared in example 1, which was activated for three cycles at a current density of 20mA/g, and then cycled 200 times at a current density of 100 mA/g.
Detailed Description
The technical solution of the present invention is further illustrated by the following embodiments in conjunction with the accompanying drawings.
Example 1:
preparing a battery comprising a high nickel ternary positive electrode material:
the first step is as follows: preparation of surface modified high-nickel ternary cathode material
A method for modifying the surface of a high-nickel ternary cathode material comprises the following steps:
s1, mixing 2g of ternary positive electrode LiNi0.83Co0.085Mn0.085O2The material is flatly paved in a quartz boat, the flatly paved thickness is controlled to be 0.5mm, the quartz boat is placed in a plasma generator, and the chamber body of the reactor is vacuumized;
s2, introducing dry carbon dioxide gas into the reactor cavity, keeping the pressure of the cavity at 550Pa for 20S, and then extracting the carbon dioxide gas to keep the vacuum degree of the cavity at 40 Pa;
and S3, starting the plasma generator, adjusting the power to 18W, and reacting for 10 minutes to obtain the surface modified high-nickel ternary cathode material.
The second step is that: preparation of the Battery
S4, weighing the obtained surface-modified high-nickel ternary positive electrode material, a conductive agent (acetylene black) and a binder (polyvinylidene fluoride) according to the mass ratio of 90:5:5, uniformly mixing, adding a proper amount of 1-methyl-2-pyrrolidone (NMP) serving as a solvent, and mechanically stirring for 3 hours to obtain slurry with a certain viscosity;
s5, uniformly coating the slurry obtained in the step S4 on a clean and smooth aluminum foil, wherein the coating thickness is 200 microns, drying the aluminum foil in a vacuum oven at 120 ℃ for 12 hours, punching the aluminum foil into a pole piece with the diameter of 15mm after drying, and compacting the pole piece with the pressure of 18MPa to serve as a positive pole piece for later use;
s6, assembling the positive electrode shell, the positive electrode plate, the diaphragm, the electrolyte, the lithium plate, the foamed nickel, the electrolyte and the negative electrode shell into the CR2025 type button cell in the glove box in sequence, wherein the model of the diaphragm is Celgard 2300, and the electrolyte is 1mol L- 1LiPF6EC + DEC (volume ratio 1: 1).
The third step: testing of electrochemical Performance
The battery prepared in the second step is placed for 12 hours and then tested for electrochemical performance:
and (3) carrying out charge and discharge tests on the battery by adopting a certain current density (the battery is activated by using a current with the current density of 20mA/g for the first 3 times, and then the battery is subjected to charge and discharge cycles by using a current with the current density of 100 mA/g), wherein the voltage interval is 3-4.2V, and the time interval of charge and discharge is 5 min. The lithium ion battery performance of the prepared material is as follows;
FIG. 1 is LiNi in the present example0.83Co0.085Mn0.085O2The SEM atlas after the ternary cathode material is treated shows that the surface of the material becomes rough after the carbon dioxide plasma treatment, but the spherical shape is not changed;
FIG. 2 is a LiNi in the present example0.83Co0.085Mn0.085O2An XRD (X-ray diffraction) spectrum of the treated ternary cathode material shows that the material layer structure is not changed after the carbon dioxide plasma treatment;
FIG. 3 is a first three-time charging and discharging curve of the battery in this embodiment with a voltage interval of 3-4.2V at a current density of 20mA/g, and a first discharge capacity of 194mA h/g;
FIG. 4 is a graph of cycle performance of the battery in this example after being activated 3 times at a current density of 20mA/g and then at a current density of 100mA/g, after 200 cycles, the discharge capacity still remained 158mA h/g, and the capacity retention rate was 86.8% (compared with the 4 th charge-discharge).
Examples 2 to 5
The procedure of example 1 was followed, with the surface treatment times varied, and the surface treatment times of examples 2-5 were 5min, 20min, 30min, and 60min (0min was the control, i.e., no surface treatment), respectively, and the procedure of assembling the cell was the same as that of example 1, and the electrochemical properties of the cell were measured as shown in table 1:
table 1: effect of carbon dioxide plasma treatment time on Material cycle Performance
From table 1, it can be seen that the ternary cathode material after the plasma surface treatment has a slight attenuation in the first discharge capacity, but has better capacity retention than the sample without the surface treatment (but is not suitable for too long time treatment), which indicates that the plasma surface modification treatment can improve the cycling stability of the material, and the treatment method provides a new idea for the surface modification treatment of the subsequent ternary cathode material.
Examples 6 to 7
The procedure for assembling the cell was the same as in example 1, except that the power of the plasma generator was changed according to the experimental procedure of example 1, the power of the plasma generator was 6.8W and 10.5W for examples 6 and 7, respectively, and the electrochemical properties of the cell were measured as shown in table 2:
table 2: effect of carbon dioxide plasma treatment Power on Material cycle Performance
From table 2, it can be seen that the high nickel ternary cathode material after plasma surface treatment has improved capacity retention rate and cycle stability compared with the high nickel ternary cathode material before plasma surface treatment, which indicates that the plasma surface modification treatment can improve the cycle stability of the material.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
Claims (5)
1. A method for modifying the surface of a high-nickel ternary cathode material is characterized by comprising the following steps:
s1, paving the high-nickel ternary positive electrode material in a quartz boat, putting the quartz boat into a cavity of the plasma generator, starting a vacuum pump, and vacuumizing the cavity of the plasma generator;
s2, introducing dry arc striking gas into the cavity, keeping the air pressure of the cavity at 500-700 Pa for 20-60S, and then extracting the arc striking gas to keep the vacuum degree of the cavity at 40-50 Pa, wherein the arc striking gas is carbon dioxide;
and S3, starting the plasma generator, adjusting the power, and reacting for 0.5-120 minutes to obtain the high-nickel ternary cathode material with the surface provided with the composite coating layer of lithium carbonate and carbon.
2. The method for surface modification of a high-nickel ternary cathode material according to claim 1, wherein the chemical formula of the high-nickel ternary cathode material is LiNi0.9Co0.05Mn0.05O2、LiNi0.8Co0.1Mn0.1O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.85Co0.1Al0.05O2Or LiNi0.5Co0.2Mn0.3O2。
3. The method for modifying the surface of the high-nickel ternary cathode material according to claim 1, wherein the tiling thickness of the high-nickel ternary cathode material in step S1 is 0.3mm to 10 mm.
4. The method for surface modification of a ternary positive electrode material with high nickel content according to claim 1, wherein the power of the plasma generator in step S3 is 5-2000W.
5. A lithium ion battery, characterized in that the lithium ion battery comprises the surface-modified high-nickel ternary cathode material prepared by the method of any one of claims 1 to 4.
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| CN201910043577.3A CN109742377B (en) | 2019-01-17 | 2019-01-17 | Method for surface modification of high-nickel ternary positive electrode material |
| PCT/CN2020/071713 WO2020147671A1 (en) | 2019-01-17 | 2020-01-13 | Method for modifying surface of high nickel ternary positive electrode material |
| JP2021540849A JP7236631B2 (en) | 2019-01-17 | 2020-01-13 | Nickel ternary positive electrode material surface modification method |
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| CN109742377B (en) * | 2019-01-17 | 2021-01-05 | 浙江工业大学 | Method for surface modification of high-nickel ternary positive electrode material |
| CN110330059B (en) * | 2019-06-25 | 2022-04-01 | 浙江工业大学 | Sintering process of high-stability lithium ion high-nickel cathode material |
| CN110350167B (en) * | 2019-06-25 | 2021-01-12 | 浙江工业大学 | Preparation process for improving cycle performance and conductivity of high-nickel cathode material |
| CN110233252A (en) * | 2019-06-25 | 2019-09-13 | 浙江工业大学 | A kind of sodium-ion battery positive material surface modifying method |
| CN110350166A (en) * | 2019-06-25 | 2019-10-18 | 浙江工业大学 | A method of improving tertiary cathode material stability and processability |
| CN110350165B (en) * | 2019-06-25 | 2021-07-23 | 浙江工业大学 | Treatment process for improving stability and conductivity of high-nickel cathode material |
| CN110714195A (en) * | 2019-08-26 | 2020-01-21 | 浙江工业大学 | Surface modification method for metal lithium |
| CN111628151A (en) * | 2020-06-09 | 2020-09-04 | 湖南长远锂科股份有限公司 | Surface modification method of ternary cathode material |
| CN111883748A (en) * | 2020-06-29 | 2020-11-03 | 华南理工大学 | Method for coating oxide film on surface of lithium ion battery anode powder material |
| CN112467066A (en) * | 2020-11-25 | 2021-03-09 | 四川虹微技术有限公司 | Pulping method of high-nickel ternary material |
| CN113044893A (en) * | 2021-03-12 | 2021-06-29 | 电子科技大学 | Method for carrying out carbon coating modification on high-nickel ternary material |
| CN113764633B (en) * | 2021-07-21 | 2023-05-09 | 广西师范大学 | Surface modified lithium ion battery positive electrode material and preparation method thereof |
| CN113764634A (en) * | 2021-08-16 | 2021-12-07 | 华中科技大学 | Preparation method of lithium fluoride in-situ coated high-nickel ternary cathode material |
| CN114229921B (en) * | 2021-12-22 | 2023-09-15 | 西南科技大学 | Al 2 O 3 -ZrO 2 Coated lithium-rich manganese-based positive electrode material and preparation method thereof |
| CN114261996B (en) * | 2021-12-24 | 2023-09-22 | 广西师范大学 | Preparation method and application of single crystal high nickel ternary material with completely modified surface |
| CN114613988B (en) * | 2022-04-01 | 2022-09-20 | 湖南桑瑞新材料有限公司 | Preparation method of high-stability ternary cathode material, ternary cathode material and lithium ion battery |
| CN114988492A (en) * | 2022-05-31 | 2022-09-02 | 西安合升汇力新材料有限公司 | Nickel-rich ternary cathode material and preparation method and application thereof |
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